JP6032504B2 - リチウム二次電池およびその製造方法 - Google Patents
リチウム二次電池およびその製造方法 Download PDFInfo
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- JP6032504B2 JP6032504B2 JP2014525770A JP2014525770A JP6032504B2 JP 6032504 B2 JP6032504 B2 JP 6032504B2 JP 2014525770 A JP2014525770 A JP 2014525770A JP 2014525770 A JP2014525770 A JP 2014525770A JP 6032504 B2 JP6032504 B2 JP 6032504B2
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- silicon
- secondary battery
- containing cyclic
- lithium secondary
- positive electrode
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- 238000004519 manufacturing process Methods 0.000 title claims description 28
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 96
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- 239000010703 silicon Substances 0.000 claims description 79
- 150000001923 cyclic compounds Chemical class 0.000 claims description 77
- -1 lithium transition metal Chemical class 0.000 claims description 57
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- 239000007774 positive electrode material Substances 0.000 claims description 51
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- 150000001875 compounds Chemical class 0.000 claims description 15
- 229910052596 spinel Inorganic materials 0.000 claims description 14
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- 125000004429 atom Chemical group 0.000 claims description 12
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Description
本出願は、2012年7月17日に出願された日本国特許出願2012-158487号に基づく優先権を主張しており、その出願の全内容は本明細書中に参照として組み入れられている。
好ましい正極活物質として、上記一般式(A1)におけるMが少なくともNiを含む化合物、例えば、次の一般式(A2):LiNipM1 qMn2−p−qO4;で表されるスピネル構造のリチウム遷移金属複合酸化物が挙げられる。ここで、0<pであり、0≦qであり、p+q<2(典型的にはp+q≦1)である。好ましい一態様では、q=0であり、0.2≦p≦0.6である。上記の含有割合(上記一般式(A2)のpで示す割合)のNiを含有させることによって、スピネル構造のLiNiMn複合酸化物(例えばLiNi0.5Mn1.5O4)の充電終止時の正極電位を高電位化(典型的には4.5V(対Li/Li+)以上に高電位化)させることができ、5V級のリチウム二次電池を構築することが可能になる。上記一般式(A2)において、0<qである場合、M1は、Ni,Mn以外の任意の金属元素または非金属元素(例えば、Fe,Co,Cu,Cr,ZnおよびAlから選択される1種または2種以上)であり得る。M1が3価のFeおよびCoの少なくとも一方を含むことが好ましい。また、0<q≦0.3であり、1≦2p+qであることが好ましい。
(3)一般式Li2MO3で表されるリチウム遷移金属複合酸化物。ここで、Mは、Mn,Fe,Co等の遷移金属元素の少なくとも1種を含み、他の金属元素または非金属元素をさらに含み得る。具体例としては、Li2MnO3,Li2PtO3等が挙げられる。
(4)一般式LiMPO4で表されるリチウム遷移金属化合物(リン酸塩)。ここで、Mは、Mn,Fe,Ni,Co等の遷移金属元素の少なくとも1種を含み、他の金属元素または非金属元素をさらに含み得る。具体例としては、LiMnPO4,LiFePO4等が挙げられる。
(5)一般式Li2MPO4Fで表されるリチウム遷移金属化合物(リン酸塩)。ここで、Mは、Mn,Ni,Co等の遷移金属元素の少なくとも1種を含み、他の金属元素または非金属元素をさらに含み得る。具体例としては、Li2MnPO4F等が挙げられる。
(6)LiMO2とLi2MO3との固溶体。ここで、LiMO2は上記(2)に記載の一般式で表される組成を指し、Li2MO3は上記(3)に記載の一般式で表される組成を指す。具体例としては、0.5LiNi1/3Mn1/3Co1/3O2−0.5Li2MnO3で表される固溶体が挙げられる。
[正極の作製]
正極活物質としてLiNi0.5Mn1.5O4粉末(NiMnスピネル)と、導電材としてアセチレンブラック(AB)と、結着材としてポリフッ化ビニリデン(PVDF)とを、これらの材料の質量比が85:10:5となるようにN−メチル−2−ピロリドン(NMP)で混合して、ペースト状の正極合材層形成用組成物を調製した。この組成物を、アルミニウム箔(厚さ15μm)の片面に塗付量が6.5mg/cm2(固形分基準)となるように均一に塗付した。その塗付物を乾燥させ、プレスした後、所定サイズ(直径14mmの円形)に切り出して正極を得た。
負極活物質としてグラファイト粉末と、結着材としてPVDFとを、これらの材料の質量比が92.5:7.5となるようにNMPで混合して、ペースト状の負極合材層形成用組成物を調製した。この組成物を、銅箔(厚さ15μm)の片面に塗付量が4.3mg/cm2(固形分基準)となるように均一に塗付した。その塗付物を乾燥させ、プレスした後、所定サイズ(直径16mmの円形)に切り出して負極を得た。
上記のようにして作製した正極と負極とを用いて、図4に示す概略構造のコイン型(2032型)電池200を作製した。すなわち、上記で作製した正極30および負極40を、非水電解液25を含浸させたセパレータ50とともに積層し、容器80(負極端子)に収容した後、さらに同電解液を滴下した。次いで、ガスケット60および蓋70(正極端子)で容器80を封止して、電池200を得た。セパレータとしては、厚み25μmのポリプロピレン(PP)製多孔質フィルムを所定サイズ(直径19mmの円形)に切り出したものを使用した。非水電解液としては、エチレンカーボネート(EC)とエチルメチルカーボネート(EMC)とジメチルカーボネート(DMC)との3:4:3(体積比)混合溶媒に、支持塩として約1mol/LのLiPF6を溶解し、さらにケイ素含有環状化合物として2,4,6,8−テトラビニル−2,4,6,8−テトラメチルシクロテトラシロキサン(4VC4S)0.5%を含有させた電解液を用いた。
ケイ素含有環状化合物の含有率(添加率)を表1に示すように代えた他は例1と同様にして例2,3に係るコイン型電池を作製した。
4VC4Sを用いなかった他は例1と同様にして例4に係るコイン型電池を作製した。
4VC4Sを表1に示す添加剤に代えた他は例1と同様にして例5〜7に係るコイン型電池を作製した。
非水電解液の非水溶媒として、EC:EMC:DMC=3:4:3(体積比)の混合溶媒に代えてジフルオロエチレンカーボネート(DFEC)とジエチルカーボネート(DEC)との1:1(体積比)混合溶媒を用いた他は例1と同様にして例8に係るコイン型電池を作製した。
4VC4Sを用いなかった他は例8と同様にして例9に係るコイン型電池を作製した。
上記で得られた各電池に対して、温度25℃にて、1/10Cのレートで4.1Vまで充電する操作と、同じレートで3.0Vまで放電させる操作とを交互に3回繰り返した。次いで、60℃の温度環境において、4.9Vまでの定電流定電圧(CCCV)充電(1Cレート、0.15Cカット)と、3.5Vまでの定電流(CC)放電(1Cレート)とを100サイクル繰り返した(サイクル試験)。1サイクル目の放電容量(初期放電容量)を100%として、100サイクル後の放電容量の維持率(%)を求めた。得られた結果を表1に示す。また、例1と例4については、サイクル数と容量維持率(%)との関係を図5に示す。
ケイ素含有環状化合物を4VC4Sから2,4,6−トリビニル−2,4,6−トリメチルシクロトリシロキサン(3VC3S)に代えた他は例1と同様にして例10に係るコイン型電池を作製した。
正極活物質として、NiMnスピネルに代えてLiMn2O4粉末(Mnスピネル)を用いた他は例1と同様にして正極を作製し、例11に係るコイン型電池を作製した。
4VC4Sを用いなかった他は例11と同様にして例12に係るコイン型電池を作製した。
例11および12に係る電池に対して、温度25℃にて、1/10Cのレートで4.1Vまで充電する操作と、同じレートで3.0Vまで放電させる操作とを交互に3回繰り返した。次いで、60℃の温度環境において、4.9VまでのCCCV充電(1Cレート、0.15Cカット)と、3.0VまでのCC放電(1Cレート)とを50サイクル繰り返した(サイクル試験)。1サイクル目の放電容量(初期放電容量)を100%として、50サイクル後の放電容量の維持率(%)を求めた。得られた結果を表3に示す。
また、例11および12に係る電池に対して、温度25℃にて、1/10Cのレートで4.1Vまで充電する操作と、同じレートで3.0Vまで放電させる操作とを交互に3回繰り返した。次いで、60℃の温度環境において、4.2VまでのCCCV充電(1Cレート、0.15Cカット)と、3.0VまでのCC放電(1Cレート)とを100サイクル繰り返した(サイクル試験)。1サイクル目の放電容量(初期放電容量)を100%として、100サイクル後の放電容量の維持率(%)を求めた。得られた結果を表3に示す。また、サイクル数と容量維持率(%)との関係を図6に示す。
正極活物質として、NiMnスピネルに代えてLiMnPO4粉末(Mnオリビン)を用いた他は例1と同様にして正極を作製し、例13に係るコイン型電池を作製した。
4VC4Sを用いなかった他は例13と同様にして例14に係るコイン型電池を作製した。
例13および14に係る電池に対して、温度25℃にて、1/10Cのレートで4.1Vまで充電する操作と、同じレートで3.0Vまで放電させる操作とを交互に3回繰り返した。次いで、60℃の温度環境において、4.8VまでのCCCV充電(1Cレート、0.15Cカット)と、2.0VまでのCC放電(1Cレート)とを100サイクル繰り返した(サイクル試験)。1サイクル目の放電容量(初期放電容量)を100%として、100サイクル後の放電容量の維持率(%)を求めた。得られた結果を表4に示す。
正極活物質として、NiMnスピネルに代えてLiNi1/3Co1/3Mn1/3O2粉末(NiCoMn層状)を用いた他は例1と同様にして正極を作製し、例15に係るコイン型電池を作製した。
4VC4Sを用いなかった他は例15と同様にして例16に係るコイン型電池を作製した。
例15および16に係る電池に対して、温度25℃にて、1/10Cのレートで4.1Vまで充電する操作と、同じレートで3.0Vまで放電させる操作とを交互に3回繰り返した。次いで、60℃の温度環境において、4.6VまでのCCCV充電(1Cレート、0.15Cカット)と、3.0VまでのCC放電(1Cレート)とを100サイクル繰り返した(サイクル試験)。1サイクル目の放電容量(初期放電容量)を100%として、100サイクル後の放電容量の維持率(%)を求めた。得られた結果を表5に示す。
ケイ素含有環状化合物を4VC4Sから2,2,4,4,6,6,8,8−オクタビニルシクロテトラシロキサン(8VC4S)に代えた他は例1と同様にして例17に係るコイン型電池を作製した。
上記で得られた例17に係る電池に対して、温度25℃にて、1/10Cのレートで4.1Vまで充電する操作と、同じレートで3.0Vまで放電させる操作とを交互に3回繰り返した(コンディショニング)。次いで、60℃の温度環境において、4.9Vまでの定電流定電圧(CCCV)充電(1Cレート、0.15Cカット)と、3.5Vまでの定電流(CC)放電(1Cレート)とを100サイクル繰り返した(サイクル試験)。1サイクル目の放電容量(初期放電容量)を100%として、100サイクル後の放電容量の維持率(%)を求めた。得られた結果を表1に示す。対比のため、例1,4に係る電池に対しても同様の試験を行った。結果を表6に示す。
例17に係る電池について、上記コンディショニング後にSOC60%の充電状態に調整したもの(サイクル試験前)の交流インピーダンス測定を行った。対比のため、例1,4に係る電池に対しても同様の試験を行った。結果を図8に示す。交流インピーダンス測定条件は、周波数範囲1MHz〜0.1Hz、電圧振幅5mVとした。
10 電池ケース
12 開口部
14 蓋体
20 捲回電極体
25 非水電解質(非水電解液)
30 正極(正極シート)
32 正極集電体
34 正極合材層
35 正極集電体積層部
36 正極合材層非形成部
37 内部正極端子
38 外部正極端子
40 負極(負極シート)
42 負極集電体
44 負極合材層
45 負極集電体積層部
46 負極合材層非形成部
47 内部負極端子
48 外部負極端子
50,50A,50B セパレータ(セパレータシート)
100 リチウム二次電池
Claims (10)
- 4.5V級以上のリチウム二次電池であって、
正極活物質として、式:LiNi p M 1 q Mn 2−p−q O 4 (式中、0<pであり、0≦qであり、p+q<2である。M 1 は、Ni,Mn以外の任意の金属元素または非金属元素である。);で表されるスピネル構造のリチウム遷移金属複合酸化物と、
非水電解液(ただし、架橋剤として、中心にオキシアルキレン基を有し、末端に少なくとも2つの(メタ)アクリル基を有する直鎖状または分枝状化合物を含むものを除く。)と、
を含み、
前記リチウム二次電池を構成する負極の表面には、ケイ素含有環状化合物の反応生成物が存在しており、
前記ケイ素含有環状化合物は、環を構成する原子がケイ素原子と酸素原子とからなり、かつ少なくとも1つのビニル基を有し、
前記非水電解液における前記ケイ素含有環状化合物の含有率は5質量%以下である、リチウム二次電池。 - 4.5V級以上のリチウム二次電池であって、
正極活物質として、式:LiNi p M 1 q Mn 2−p−q O 4 (式中、0<pであり、0≦qであり、p+q<2である。M 1 は、Ni,Mn以外の任意の金属元素または非金属元素である。);で表されるスピネル構造のリチウム遷移金属複合酸化物と、
非水電解液(ただし、架橋剤として、中心にオキシアルキレン基を有し、末端に少なくとも2つの(メタ)アクリル基を有する直鎖状または分枝状化合物を含むものを除く。)と、
を含み、
前記非水電解液は、ケイ素含有環状化合物を含み、
前記ケイ素含有環状化合物は、環を構成する原子がケイ素原子と酸素原子とからなり、かつ少なくとも1つのビニル基を有し、
前記非水電解液における前記ケイ素含有環状化合物の含有率は5質量%以下である、リチウム二次電池。 - 前記ケイ素含有環状化合物は、環を構成するケイ素原子に結合した置換基がすべてビニル基である、請求項1〜3のいずれか一項に記載のリチウム二次電池。
- 前記非水電解液は、非水溶媒としてフッ素化カーボネートを含む、請求項1〜4のいずれか一項に記載のリチウム二次電池。
- 4.5V級以上のリチウム二次電池を製造する方法であって、
正極活物質としてリチウム遷移金属複合酸化物を含む正極と負極とを用意すること、および
少なくとも前記負極にケイ素含有環状化合物を供給すること、を包含し、
前記リチウム二次電池は、非水電解液(ただし、架橋剤として、中心にオキシアルキレン基を有し、末端に少なくとも2つの(メタ)アクリル基を有する直鎖状または分枝状化合物を含むものを除く。)を含み、
前記ケイ素含有環状化合物は、環を構成する原子がケイ素原子と酸素原子とからなり、かつ少なくとも1つのビニル基を有し、
前記ケイ素含有環状化合物の供給は、
前記ケイ素含有環状化合物を含む前記非水電解液を用意すること、および
前記用意した非水電解液を、前記正極と前記負極とを備える電極体に供給すること、
を包含し、
前記正極活物質は、式:LiNi p M 1 q Mn 2−p−q O 4 (式中、0<pであり、0≦qであり、p+q<2である。M 1 は、Ni,Mn以外の任意の金属元素または非金属元素である。);で表されるスピネル構造のリチウム遷移金属複合酸化物であり、
前記非水電解液における前記ケイ素含有環状化合物の含有率は5質量%以下である、リチウム二次電池の製造方法。 - 前記ケイ素含有環状化合物は、環を構成するケイ素原子に結合した置換基がすべてビニル基である、請求項6または7に記載のリチウム二次電池の製造方法。
- 前記非水電解液の非水溶媒として、フッ素化カーボネートを用いる、請求項6〜8のいずれか一項に記載のリチウム二次電池の製造方法。
- 請求項1〜5のいずれか一項に記載のリチウム二次電池を搭載した車両。
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